CN101475646B - Method for preparing acetate starch by microwave and infrared heating - Google Patents
Method for preparing acetate starch by microwave and infrared heating Download PDFInfo
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- CN101475646B CN101475646B CN2008102333051A CN200810233305A CN101475646B CN 101475646 B CN101475646 B CN 101475646B CN 2008102333051 A CN2008102333051 A CN 2008102333051A CN 200810233305 A CN200810233305 A CN 200810233305A CN 101475646 B CN101475646 B CN 101475646B
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Abstract
The invention relates to a method for preparing acetate starch through microwave and infrared heating. The method which integrates a microwave rapid temperature rising heating mode and an infrared high efficiency temperature control mode can overcome the defects that though the temperature is quickly raised, the microwave heating mode has the poor temperature stability and difficult control, thereby making the microwave and infrared heating energy-saving technology be applied to the field of modified starch production in a truly large scale. The method cannot only overcome the defect of unstable product quality for pure microwave heating, but also realize high efficiency, energy conservation, emission reduction and consumption reduction. The production time can be saved by 60 to 90 percent without wastewater treatment and emission. The dosage of supplementary chemical materials used for the reaction can be reduced by 20 to 40 percent.
Description
Technical field
The present invention relates to technical fields such as food-processing and weaving, papermaking, particularly relate to a kind of preparation method of acetic ester modified starch.
Background technology
Modified starch is one of product of starch deep processing, and chemical modification, physical modification and enzyme denaturation starch are arranged, and wherein chemically modified starch has accounted for more than 2/3 of total amount, and the production of development modified starch is the important component part of starch industry development.The production of modified starch is to utilize starch and various chemical reagent (chemical modification) under the uniform state of thorough mixing, reacts at a certain temperature.In wet process technique, 1 ton of modified starch of every production approximately will consume the water of 2-3 ton, and this part water is finally converted into the difficult sewage of COD and salt content height (saltiness of some kind has reached the saliferous degree of seawater), causes serious environmental to pollute.Applying of dry production technology not only can be improved the production efficiency of modified starch, reduces production costs, and improves the quality of products, diversify, and conserve water resource and reduce environmental pollution in a large number.In the dry process reaction,, suppressed side reaction to greatest extent owing to have only the intervention of a small amount of solvent molecule, in addition, the intervention of a small amount of solvent molecule makes the microenvironment of reaction system be different from liquid phase reaction, has caused the high local concentrations of reactive site, has improved reaction efficiency greatly.Can avoid because of the high energy consumption of using a large amount of solvents to cause, environmental pollution, toxic etc., be a kind of energy-conservation, eco-friendly technology.Another characteristics of dry method are to prepare the high substitution value modified starch that wet method can't prepare, thereby can widen the Application Areas of modified starch.The preparation that new and effective solid phase heating technique is applied to modified starch is a research focus current and from now on.
Acetate starch is acetylated starch again, is hydroxyl direct under certain condition and acetic acid reaction or a kind of starch derivative indirect and that the acetic acid derivative reaction obtains in the starch polymer.Compare it with ative starch and have characteristics such as gelatinization point is low, viscosity is big, transparency is good, retrogradation weakens, good film-forming property, can be widely used in fields such as food, weaving, papermaking.The preparation method of acetate starch has the physics method, is meant to utilize physical condition (as microwave radiation, ultraviolet radiation, gamma-rays radiation etc.) initiation reaction to carry out; Chemical method is meant the product that the free radical reaction of utilizing chemical initiator to make ethanoyl and starch obtains.
Wherein microwave technology fast, energy-conservation with its rate of heating, save time, simplify procedures, reduce organic solvent and use, improve advantages such as speed of reaction, system be easy to control, be incorporated in the preparation of modified starch, now be in experimental study and exploratory stage, also do not realize the suitability for industrialized production application.Studied with dry microwave as Zhang Yonghua etc. and to have prepared acetate starch.Taking by weighing water content is put in the mixing tank that homogenizer is housed less than 3% starch, 60 grams.Take by weighing CHPTMA 30 grams and be dissolved in 12 ml waters, take by weighing 11 gram sodium hydroxide and be dissolved in 11 ml waters.After treating that two solution mix, be added in the mixing tank, and constantly stir and make itself and starch mixing in the mode of spraying.With the microwave oven heating 5 to 6 minutes that mixture places 800 watts of power, be 6.5～7.5 with the hydrochloric acid neutralization up to pH, use then air-flow air-dry to its water content less than 14%, get product.Zhao Haibo, Ma Tao etc. have been studied the microwave wet method and have been prepared acetate starch.At first, take by weighing over dry starch 20 and restrain in mortar, get certain density sodium hydroxide solution and the abundant mixing of a certain amount of water, regulate pH with hydrochloric acid soln then.Starch and mixed solution transfer are put in the microwave reactor, treated that condensing works connects, and behind the logical water of condensation, open agitator, in separating funnel, add acetic anhydride then, select irradiation power to carry out esterification.Product washing after the reaction end is poured in the culture dish after being slightly acidic, and freeze-day with constant temperature to constant weight promptly gets sample.
Microwave is that frequency is at the hertzian wave (wavelength 1 meter-1 millimeter) of 300 megahertzes to 300 mega hertzs.The material medium is by polar molecule and non-polar molecule tissue, and under electromagnetic field effect, these polar molecules transfer to according to direction of an electric field from the stochastic distribution state and carry out orientations.And under the microwave electromagnetic field action, these orientation movements constantly change with the billions of inferior frequencies of per second, cause the strenuous exercise and the collision friction of molecule, thereby produce heat, reach electric energy and are converted into the interior heat energy of medium.Therefore, microwave heating is dielectric material own loss electric field energy and generating heat.Microwave application has following advantage in modified starch processing: microwave heating is to carry out surface and inner consistent integral body heating by micro-wave energy and starch direct interaction, and rate of heating is fast, the time is short, quality product is high, homogeneous heating.And heat-processed has the automatic thermal balance performance, be quick on the draw to be easy to control, and the thermo-efficiency height, occupation area of equipment is few etc.Efficient and the homogeneity of microwave heating is the number affects that is subjected to reaction mass Semi-polarity molecule, in starch material, mainly is the influence of moisture content.
Owing to microwave heating is to rely on the polar molecule absorption microwave generation vibration in the heated material to generate heat, be in the heating top layer starch granules in moisture evaporation fast, when water content is lower than 5%, need bigger thermal value to support the intensification of polar molecule, or there are not enough polar molecules to support the persistent fever of top layer starch granules, cause its temperature lower than the starch granules that is in middle level and bottom all the time, also cause when reacting with chemical reagent, the reaction denaturation degrees is influenced.Be in the starch of nexine because moisture evaporation is slow, and moisture content is higher, easily the microwave radiation of hyperabsorption can cause the starch quick heating and height, produces burnt phenomenon of sticking with paste.And existing industrialized microwave heating thermometric is to adopt infrared technique, can only the searching surface material temperature, can't obtain the temperature of internal layer.This also is that microwave technology can not be used for the major cause of suitability for industrialized production so far.
Infrared Heating is the power-saving technology that country applies, and it can make the whole space of its heating keep the temperature of required control, has good insulation effect.But its thermo-efficiency is lower than microwave heating.The rapid heating of microwave is combined with infrared efficient heat energy temperature control, be applied to the preparation of acetate starch, can reach efficient, energy-conservation, reduce discharging, the effect of consumption reduction.Still there is not the correlative study report both at home and abroad.
Summary of the invention
The objective of the invention is to propose a kind of quick, energy-conservation acetic ester method for preparing modified starch; this method combines the type of heating that is rapidly heated of microwave with infrared efficiently controlling temperature mode; though can overcome the microwave heating quick heating; but temperature stability difference and the difficult shortcoming of control make microwave, Infrared Heating power-saving technology real mass-producing be applied to the modified starch production field.The thermo-efficiency of microwave heating and Infrared Heating is variant, so the preparation technology parameter of acetate starch is not merely the continuity of microwave reaction process, but under different type of heating, need adjust processing parameter.
The objective of the invention is to realize by following technological line: with starch (can be W-Gum, yam starch, tapioca (flour), sweet potato starch etc., wherein any one) thorough mixing is even according to a certain percentage with the chemical reagent that reacts, through predrying or damping, the moisture content of compound is controlled within the specific limits, it is temperature required to reaction in microwave heating installation compound to be rapidly heated, the compound that will heat by travelling belt is transported in the Infrared Heating chamber that is preheating to the reaction design temperature, behind the insulation certain hour, the product that reaction is finished washs to being slightly acidic, and freeze-day with constant temperature is to moisture content about 13.5%.
Microwave of the present invention, Infrared Heating prepare the method for acetate starch, realize by following process steps:
Take by weighing a certain amount of starch, the sodium hydroxide that adds starch quality 1/30～1/15, in the high-speed mixer of 1000rpm～4000rpm with its stirring and evenly mixing, then acetic anhydride is sprayed in the mixture of starch and sodium hydroxide, the consumption of acetic anhydride is: acetic anhydride: starch=(0.4-0.2): 1 volume mass is than (v/w, liter/kilogram), stir while spraying, after stirring, send in the belt microwave reactor, in in 20～180 seconds temperature risen to 60 ℃～90 ℃ design temperature, utilize conveying belt then, the reaction mass that rises to design temperature is transported in the Infrared heaters that has risen to design temperature fast reacts, the temperature of Infrared heaters is set higher by 3%～15% than microwave heater, this section heat tracing reaction 10～25 minutes, material that the material that reaction is finished produces with the side reaction of deionized water flush away and the acetic anhydride that has neither part nor lot in reaction, behind the repeated washing three times, the elimination washing lotion, filter cake pulverized in the pneumatic drier enter 45 ℃～70 ℃ dry, and remove the modified starch particle of big conglomeration through 100 mesh sieves, screen overflow returns into pulverizer and pulverizes again, and screen underflow is the modified starch that conforms to quality requirements.
Substitution value with the acetate starch of the inventive method preparation is 0.03～0.25.
The present invention has the following advantages:
1, microwave and infrared heating technique are applied to the suitability for industrialized production of modified starch, realized efficient, energy-conservation, reduce discharging, consumption reduction.
2, by the combining of microwave heating and infrared heating technique, it is difficult to have overcome simple microwave heating temperature control, the shortcoming of unstable product quality.
3, the production time can save 60%～90%, does not have the processing and the discharging of waste water, and the change auxiliary material that is used to react can reduce by 20%～40% consumption.
Embodiment:
Embodiment 1:
Take by weighing 500 kilograms of starch, the sodium hydroxide that adds 17 kilograms, in the mixing machine of 1000rpm with its stirring and evenly mixing, get 100 liters of acetic anhydride, it is sprayed in the mixture of starch and sodium hydroxide, stir while spraying, after stirring, send in the microwave reactor, temperature is risen to 60 ℃ design temperature in 20 seconds, utilize conveying belt, reaction mass is transported to fast the Infrared heaters that has been warming up to 66 ℃, heat tracing reaction 10 minutes, after the material that reaction is finished finishes for 3 times with deionized water wash, the elimination washing lotion, filter cake pulverized in the pneumatic drier enter 70 ℃ dry, and remove the modified starch particle of big conglomeration through 100 mesh sieves, and screen overflow returns into pulverizer and pulverizes again, and screen underflow is the modified starch that conforms to quality requirements.After measured, the substitution value of gained acetate starch is 0.06.
Embodiment 2:
Take by weighing 500 kilograms of starch, the sodium hydroxide that adds 25 kilograms, in the mixing machine of 3000rpm with its stirring and evenly mixing, get 150 liters of acetic anhydride, it is sprayed in the mixture of starch and sodium hydroxide, stir while spraying, after stirring, send in the microwave reactor, temperature is risen to 70 ℃ design temperature in 40 seconds, utilize conveying belt, reaction mass is transported to fast the Infrared heaters that has been warming up to 80 ℃, heat tracing reaction 20 minutes, after the material that reaction is finished finishes for 3 times with deionized water wash, the elimination washing lotion, filter cake pulverized in the pneumatic drier enter 60 ℃ dry, and remove the modified starch particle of big conglomeration through 100 mesh sieves, and screen overflow returns into pulverizer and pulverizes again, and screen underflow is the modified starch that conforms to quality requirements.After measured, the substitution value of gained acetate starch is 0.16.
Embodiment 3:
Take by weighing 500 kilograms of starch, the sodium hydroxide that adds 34 kilograms, in the mixing machine of 4000rpm with its stirring and evenly mixing, get 200 liters of acetic anhydride, it is sprayed in the mixture of starch and sodium hydroxide, stir while spraying, after stirring, send in the microwave reactor, temperature is risen to 90 ℃ design temperature in 180 seconds, utilize conveying belt, reaction mass is transported to fast the Infrared heaters that has been warming up to 93 ℃, heat tracing reaction 25 minutes, after the material that reaction is finished finishes for 3 times with deionized water wash, the elimination washing lotion, filter cake pulverized in the pneumatic drier enter 45 ℃ dry, and remove the modified starch particle of big conglomeration through 100 mesh sieves, and screen overflow returns into pulverizer and pulverizes again, and screen underflow is the modified starch that conforms to quality requirements.After measured, the substitution value of gained acetate starch is 0.25.
Claims (1)
1. microwave, Infrared Heating prepare the method for acetate starch, it is characterized in that realizing by following process steps:
Take by weighing a certain amount of starch, the sodium hydroxide that adds starch quality 1/30～1/15, in the high-speed mixer of 1000rpm～4000rpm with its stirring and evenly mixing, then acetic anhydride is sprayed in the mixture of starch and sodium hydroxide, the consumption of acetic anhydride is: acetic anhydride: starch=(0.4-0.2): 1 volume mass ratio, stir while spraying, after stirring, send in the belt microwave reactor, in in 20～180 seconds temperature risen to 60 ℃～90 ℃ design temperature, utilize conveying belt then, the reaction mass that rises to design temperature is transported in the Infrared heaters that has risen to design temperature fast reacts, the temperature of Infrared heaters is set higher by 3%～15% than microwave heater, this section heat tracing reaction 10～25 minutes, material that the material that reaction is finished produces with the side reaction of deionized water flush away and the acetic anhydride that has neither part nor lot in reaction, behind the repeated washing three times, the elimination washing lotion, filter cake pulverized in the pneumatic drier enter 45 ℃～70 ℃ dry, and remove the modified starch particle of big conglomeration through 100 mesh sieves, screen overflow returns into pulverizer and pulverizes again, and screen underflow is the modified starch that conforms to quality requirements;
The volume mass ratio is v/w, liter/kilogram.
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| CN2008102333051A CN101475646B (en) | 2008-12-11 | 2008-12-11 | Method for preparing acetate starch by microwave and infrared heating |
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| CN101475646A CN101475646A (en) | 2009-07-08 |
| CN101475646B true CN101475646B (en) | 2010-10-20 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103739724B (en) * | 2014-01-14 | 2016-08-17 | 山东渠风食品科技有限公司 | Semen Tritici aestivi flour extracts the method for the A Starch Production acetate starch after gluten meal |
| CN103897068A (en) * | 2014-04-02 | 2014-07-02 | 枣庄超越玉米淀粉有限公司 | Efficient energy-saving production method of modified starch |
| CN103980097B (en) * | 2014-05-21 | 2016-06-22 | 芜湖职业技术学院 | A kind of synthetic method of phenols etherificate |
| CN104817708B (en) * | 2015-04-17 | 2017-04-05 | 江南大学 | It is a kind of to improve starch packaging paper of microwave heating and preparation method thereof |
| CN105384833A (en) * | 2015-12-15 | 2016-03-09 | 陈虹 | Water chestnut starch acetate and preparation method thereof |
| CN111234042B (en) | 2020-01-17 | 2021-06-22 | 南京财经大学 | Preparation method of citric acid modified starch with anti-digestion characteristic |
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